CN112811470A - Method for preparing high-purity uranyl fluoride powder from uranium hexafluoride by dry method - Google Patents
Method for preparing high-purity uranyl fluoride powder from uranium hexafluoride by dry method Download PDFInfo
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- CN112811470A CN112811470A CN202011314015.7A CN202011314015A CN112811470A CN 112811470 A CN112811470 A CN 112811470A CN 202011314015 A CN202011314015 A CN 202011314015A CN 112811470 A CN112811470 A CN 112811470A
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- uranium hexafluoride
- gas
- reaction
- water vapor
- dry method
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- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 57
- KCKICANVXIVOLK-UHFFFAOYSA-L dioxouranium(2+);difluoride Chemical compound [F-].[F-].O=[U+2]=O KCKICANVXIVOLK-UHFFFAOYSA-L 0.000 title claims abstract description 44
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 94
- 230000001681 protective effect Effects 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000003758 nuclear fuel Substances 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910000442 triuranium octoxide Inorganic materials 0.000 description 1
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 description 1
- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G43/00—Compounds of uranium
Abstract
The invention belongs to the technical field of nuclear fuel element manufacturing, and particularly relates to a method for preparing high-purity uranyl fluoride powder by a uranium hexafluoride dry method, which comprises the following steps of firstly, heating and gasifying the uranium hexafluoride in a container to obtain uranium hexafluoride gas; heating uranium hexafluoride gas and water vapor and then continuously introducing the heated uranium hexafluoride gas and the water vapor into a reaction furnace; step three, carrying out gas-phase hydrolysis reaction on uranium hexafluoride gas and water vapor in a reaction furnace to generate uranyl fluoride powder; fourthly, the generated uranyl fluoride powder is produced by a discharging device of the reaction furnace, and tail gas generated in the reaction process is discharged by an exhaust device of the reaction furnace; the method can realize that the uranyl fluoride powder is obtained by using uranium hexafluoride as a raw material and performing a gas phase hydrolysis dry reaction through contact between uranium hexafluoride gas and water vapor, can complete conversion of the uranium hexafluoride gas to prepare uranyl fluoride in one step, and can be continuously performed. Compared with the traditional wet process, the preparation process is greatly shortened, the production continuity is improved, and the material yield is improved.
Description
Technical Field
The invention belongs to the technical field of nuclear fuel element manufacturing, and particularly relates to a method for preparing high-purity uranyl fluoride powder by a uranium hexafluoride dry method.
Background
The uranyl fluoride powder is an important intermediate product in the manufacturing process of nuclear fuel elements, and can be used for preparing uranium dioxide, triuranium octoxide, uranium tetrafluoride and the like through conversion. At present, depleted or concentrated uranium hexafluoride is mostly used as a raw material for preparing uranyl fluoride powder, and at present, uranyl fluoride is mostly prepared by a wet production process, and uranium hexafluoride is converted into uranyl fluoride through wet treatment. The uranyl fluoride powder is obtained by gasifying uranium hexafluoride, introducing the gasified uranium hexafluoride into water to generate a uranyl fluoride aqueous solution, heating to evaporate water, and drying by a fluidized bed.
The wet preparation process has the defects of long process flow, low material yield, high critical risk, low automation degree, low productivity and the like, and meanwhile, the uranyl fluoride powder obtained by the process has poor fluidity and low purity, and is difficult to be used for preparing other products by conversion.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a method for preparing high-purity uranyl fluoride powder by a dry uranium hexafluoride method, which can shorten the preparation process of uranyl fluoride, improve productivity, improve material yield, and reduce critical safety risk. In addition, the method can realize continuous production and can be widely applied to the field of uranium chemical conversion.
The technical scheme of the invention is as follows:
a method for preparing high-purity uranyl fluoride powder by a uranium hexafluoride dry method comprises the steps of firstly, heating and gasifying uranium hexafluoride in a container to obtain uranium hexafluoride gas;
heating uranium hexafluoride gas and water vapor and then continuously introducing the heated uranium hexafluoride gas and the water vapor into a reaction furnace;
step three, carrying out gas-phase hydrolysis reaction on uranium hexafluoride gas and water vapor in a reaction furnace to generate uranyl fluoride powder;
fourthly, the generated uranyl fluoride powder is produced by a discharging device of the reaction furnace, and tail gas generated in the reaction process is discharged by an exhaust device of the reaction furnace;
the uranium hexafluoride in the step one can be any enrichment material within the safety range related to equipment.
In the first step, uranium hexafluoride is heated and gasified, the gasification temperature is 70-120 ℃, and the gas outlet pressure of a uranium hexafluoride container is 0.1-0.4 MPa.
The uranium hexafluoride gas and the water vapor in the second step are transmitted by adopting a pipeline and are independently transmitted without contacting each other before entering the reaction furnace;
heating the uranium hexafluoride gas and the water vapor before introducing the uranium hexafluoride gas and the water vapor into the reaction chamber, wherein the heating temperature is 140-220 ℃;
the pressure of a gas pipeline before introducing the uranium hexafluoride gas and the water vapor into the reaction furnace is 0-100 kpa.
And (2) introducing the uranium hexafluoride gas and the water vapor in the second step into the reaction chamber in a concentric circle mode, wherein the uranium hexafluoride gas is an inner ring, and the water vapor is an outer ring.
And the flow ratio of the uranium hexafluoride gas and the steam introduced in the step II is that the mass ratio of the uranium hexafluoride gas to the steam is 1.5-4: 1.
the uranium hexafluoride gas and the water vapor are subjected to gas phase hydrolysis reaction in a reaction furnace, and the reaction temperature is 150-300 ℃;
the gas-phase hydrolysis reaction of the uranium hexafluoride gas and the water vapor occurs in the reaction furnace, and the reaction pressure is-10 to 30 kpa.
Inert gases such as nitrogen and the like can be introduced for protection in the reaction process in the third step, and the flow proportion of the protective gases is as follows: the mass ratio of the uranium hexafluoride gas to the protective gas is 1.5-4: 1, introducing protective gas into a pipeline at the pressure of 0-100 kpa, and controlling the temperature of the protective gas at 140-220 ℃.
And the reaction furnace, the discharging device and the exhaust device in the fourth step are made of materials which are resistant to hydrogen fluoride corrosion and high temperature, such as NS331 and NCu 30.
The reaction furnace in the fourth step is a horizontal furnace or a shaft furnace.
And the reaction furnace in the fourth step is provided with a rapping device.
The invention has the beneficial effects that:
the method can realize that the uranyl fluoride powder is obtained by using uranium hexafluoride as a raw material and performing a gas phase hydrolysis dry reaction through contact between uranium hexafluoride gas and water vapor, can complete conversion of the uranium hexafluoride gas to prepare uranyl fluoride in one step, and can be continuously performed. Compared with the traditional wet process, the preparation process is greatly shortened, the production continuity is improved, and the material yield is improved. The method can be applied to the dry preparation of uranyl fluoride powder by taking uranium hexafluoride as a raw material in the fields of nuclear chemical industry and fuel element manufacturing.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing high-purity uranyl fluoride powder by a uranium hexafluoride dry method. The method comprises the following steps: step one, heating and gasifying uranium hexafluoride in a container to obtain uranium hexafluoride gas;
heating uranium hexafluoride gas and water vapor and then continuously introducing the heated uranium hexafluoride gas and the water vapor into a reaction furnace;
step three, carrying out gas-phase hydrolysis reaction on uranium hexafluoride gas and water vapor in a reaction furnace to generate uranyl fluoride powder;
and fourthly, the generated uranyl fluoride powder is produced by a discharging device of the reaction furnace, and tail gas generated in the reaction process is discharged by an exhaust device of the reaction furnace.
The uranium hexafluoride in the step one can be any enrichment material within the safety range related to equipment.
And step one, heating and gasifying the uranium hexafluoride, wherein the gasification temperature is (70-120) DEG C, and the gas outlet pressure of a uranium hexafluoride container is (0.1-0.4) MPa.
And the uranium hexafluoride gas and the water vapor in the step two are transmitted by adopting a pipeline and are independently transmitted without contacting each other before entering the reaction furnace.
And step two, heating the uranium hexafluoride gas and the water vapor before introducing the uranium hexafluoride gas and the water vapor into the reaction chamber, wherein the heating temperature is 140-220 ℃.
And the pressure of a gas pipeline before the uranium hexafluoride gas and the water vapor are introduced into the reaction furnace is (0-100) kpa.
And step two, introducing uranium hexafluoride gas and water vapor into the reaction chamber in a concentric circle mode, wherein the uranium hexafluoride gas is an inner ring, and the water vapor is an outer ring.
And the flow ratio of the uranium hexafluoride gas to the steam introduced in the step two is as follows: the mass ratio of the uranium hexafluoride gas to the water vapor is (1.5-4): 1.
and thirdly, carrying out gas-phase hydrolysis reaction on the uranium hexafluoride gas and water vapor in a reaction furnace, wherein the reaction temperature is (150-300 ℃).
And thirdly, carrying out gas-phase hydrolysis reaction on the uranium hexafluoride gas and water vapor in a reaction furnace, wherein the reaction pressure is (-10-30) kpa.
Inert gases such as nitrogen and the like can be introduced for protection in the reaction process in the third step, and the flow proportion of the protective gases is as follows: the mass ratio of the uranium hexafluoride gas to the protective gas is (1.5-4): 1, the pressure of the protective gas inlet pipeline is (0-100) kpa, and the temperature of the protective gas is (140-220) DEG C.
And fourthly, the reaction furnace, the discharging device and the exhaust device are made of materials with resistance to hydrogen fluoride corrosion and high temperature, such as NS331, NCu30 and the like.
The reaction furnace in the step four can be a horizontal furnace or a shaft furnace, and has good sealing property.
And fourthly, arranging a rapping device in the reaction furnace to prevent the materials from sticking to the wall.
Example 1:
the method is characterized in that the uranyl fluoride powder is prepared by adopting depleted uranium hexafluoride, the reaction furnace is a horizontal reaction furnace, the top of the reaction furnace is provided with an exhaust device, and the bottom of the reaction furnace is provided with a discharge device.
Step one, heating a uranium hexafluoride container at the temperature of 100 ℃ to gasify the uranium hexafluoride into uranium hexafluoride gas, so that the pressure of the gas at the outlet of the container reaches 200 kpa.
Step two, respectively transmitting the uranium hexafluoride gas and the water vapor by adopting pipelines, and heating the pipelines by adopting electric tracing bands to enable the temperature of the uranium hexafluoride gas and the water vapor to reach 150 ℃; introducing uranium hexafluoride gas and water vapor into the reaction furnace through a double-annular-gap concentric circular nozzle, wherein the inner annular gap is uranium hexafluoride gas, and the outer annular gap is water vapor; the pressure of the uranium hexafluoride gas and the water vapor pipeline is 50 kpa; the mass ratio of the uranium hexafluoride gas to the steam is 2: 1.
and step three, continuously introducing uranium hexafluoride gas and water vapor into a reaction furnace, and carrying out gas phase hydrolysis reaction in the reaction furnace, wherein the heating temperature of the reaction furnace is 150 ℃, and the reaction pressure is 1 kpa.
And fourthly, the uranyl fluoride powder generated by the reaction is produced by a discharging device at the bottom of the reaction furnace, the tail gas generated by the reaction is discharged by an exhaust device at the top of the reaction furnace, the whole reaction is stably carried out, and the reaction furnace can continuously produce the uranyl fluoride powder.
Example 2:
the method is characterized in that the uranyl fluoride powder is prepared by adopting depleted uranium hexafluoride, the reaction furnace is a horizontal reaction furnace, the top of the reaction furnace is provided with an exhaust device, and the bottom of the reaction furnace is provided with a discharge device.
Step one, heating a uranium hexafluoride container at the temperature of 100 ℃ to gasify the uranium hexafluoride into uranium hexafluoride gas, so that the pressure of the gas at the outlet of the container reaches 150 kpa.
Step two, respectively transmitting the uranium hexafluoride gas and the water vapor by adopting pipelines, and heating the pipelines by adopting electric tracing bands to ensure that the temperature of the uranium hexafluoride gas and the water vapor reaches 200 ℃; introducing uranium hexafluoride gas and water vapor into the reaction furnace through a double-annular-gap concentric circular nozzle, wherein the inner annular gap is uranium hexafluoride gas, and the outer annular gap is water vapor; the pressure of the uranium hexafluoride gas and the water vapor pipeline is 10 kpa; the mass ratio of the uranium hexafluoride gas to the steam is 1.5: 1.
and step three, continuously introducing uranium hexafluoride gas and water vapor into a reaction furnace, and carrying out gas phase hydrolysis reaction in the reaction furnace, wherein the heating temperature of the reaction furnace is 250 ℃, and the reaction pressure is 20 kpa.
And fourthly, the uranyl fluoride powder generated by the reaction is produced by a discharging device at the bottom of the reaction furnace, the tail gas generated by the reaction is discharged by an exhaust device at the top of the reaction furnace, the whole reaction is stably carried out, and the reaction furnace can continuously produce the uranyl fluoride powder.
The disclosed embodiment of the invention only relates to the methods related to the disclosed embodiment, other methods can refer to common design, and the same embodiment and different embodiments of the invention can be combined with each other under the condition of no conflict;
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing high-purity uranyl fluoride powder by a uranium hexafluoride dry method comprises the steps of firstly, heating and gasifying uranium hexafluoride in a container to obtain uranium hexafluoride gas;
heating uranium hexafluoride gas and water vapor and then continuously introducing the heated uranium hexafluoride gas and the water vapor into a reaction furnace;
step three, carrying out gas-phase hydrolysis reaction on uranium hexafluoride gas and water vapor in a reaction furnace to generate uranyl fluoride powder;
fourthly, the generated uranyl fluoride powder is produced by a discharging device of the reaction furnace, and tail gas generated in the reaction process is discharged by an exhaust device of the reaction furnace;
the method is characterized in that:
the uranium hexafluoride in the step one can be any enrichment material within the safety range related to equipment.
2. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: in the first step, uranium hexafluoride is heated and gasified, the gasification temperature is 70-120 ℃, and the gas outlet pressure of a uranium hexafluoride container is 0.1-0.4 MPa.
3. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: the uranium hexafluoride gas and the water vapor in the second step are transmitted by adopting a pipeline and are independently transmitted without contacting each other before entering the reaction furnace;
heating the uranium hexafluoride gas and the water vapor before introducing the uranium hexafluoride gas and the water vapor into the reaction chamber, wherein the heating temperature is 140-220 ℃;
the pressure of a gas pipeline before introducing the uranium hexafluoride gas and the water vapor into the reaction furnace is 0-100 kpa.
4. The method for preparing high-purity uranyl fluoride powder by a dry method from uranium hexafluoride according to claim 3, wherein the dry method comprises the following steps: and (2) introducing the uranium hexafluoride gas and the water vapor in the second step into the reaction chamber in a concentric circle mode, wherein the uranium hexafluoride gas is an inner ring, and the water vapor is an outer ring.
5. The method for preparing high-purity uranyl fluoride powder by a dry method from uranium hexafluoride according to claim 4, wherein the dry method comprises the following steps: and the flow ratio of the uranium hexafluoride gas and the steam introduced in the step II is that the mass ratio of the uranium hexafluoride gas to the steam is 1.5-4: 1.
6. the method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: the uranium hexafluoride gas and the water vapor are subjected to gas phase hydrolysis reaction in a reaction furnace, and the reaction temperature is 150-300 ℃;
the uranium hexafluoride gas and the water vapor are subjected to gas phase hydrolysis reaction in a reaction furnace, and the reaction pressure is-10-30 kpa.
7. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: inert gases such as nitrogen and the like can be introduced for protection in the reaction process in the third step, and the flow proportion of the protective gases is as follows: the mass ratio of the uranium hexafluoride gas to the protective gas is 1.5-4: 1, introducing protective gas into a pipeline at the pressure of 0-100 kpa, and controlling the temperature of the protective gas at 140-220 ℃.
8. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: and the reaction furnace, the discharging device and the exhaust device in the fourth step are made of materials which are resistant to hydrogen fluoride corrosion and high temperature, such as NS331 and NCu 30.
9. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: the reaction furnace in the fourth step is a horizontal furnace or a shaft furnace.
10. The method for preparing high-purity uranyl fluoride powder from uranium hexafluoride through a dry method according to claim 1, wherein the dry method comprises the following steps: and the reaction furnace in the fourth step is provided with a rapping device.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011314015.7A CN112811470A (en) | 2020-11-20 | 2020-11-20 | Method for preparing high-purity uranyl fluoride powder from uranium hexafluoride by dry method |
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| CN202011314015.7A CN112811470A (en) | 2020-11-20 | 2020-11-20 | Method for preparing high-purity uranyl fluoride powder from uranium hexafluoride by dry method |
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